Method and apparatus for precursor gas injection

Abstract

The present disclosure provides a gas injection system that may include a housing configured to contain a plurality of precursor storage tanks, the plurality of precursor storage tanks including one or more precursor materials; and a nozzle extending from the housing, the nozzle having a tip configured for insertion into a sample chamber of a material processing apparatus. A precursor tank is fluidly connected with the nozzle to selectively deliver one or more precursor gases into the sample chamber.

Description

[0001] This application is a continuation-in-part of the invention patent application entitled “Method and Apparatus for Precursor Gas Injection,” International Application No. PCT / US2020 / 045988, filed August 12, 2020, and U.S. Non-Provisional Application No. 202080063778.0, filed August 12, 2020.

[0002] Related Applications

[0003] This application claims the benefit of and priority to U.S. Provisional Application No. 63 / 035,074, filed June 5, 2020, U.S. Provisional Application No. 62 / 885,795, filed August 12, 2019, and U.S. Utility Application No. 16 / 991,871, filed August 12, 2020, and the contents of these applications are hereby incorporated by reference in their entirety. TECHNICAL FIELD

[0004] The present disclosure relates generally to gas injection systems. BACKGROUND

[0005] Focused ion beam (FIB) systems, electron beam systems (such as scanning electron microscopes (SEMs)), dual-beam FIB / SEM systems, and other laser beam-based systems are used, among other uses, to deposit compounds on sample surfaces by a beam-induced deposition process. Briefly, a precursor gas containing a desired compound or a combination of gases capable of producing the desired compound as a chemical reaction is introduced into a sample chamber of the instrument where the precursor gas is subjected to decomposition or chemical reaction induced by a corresponding light beam and deposits the desired compound on the sample surface. FIB, SEM, dual-beam FIB / SEM, and laser-based systems can utilize a gas injection system (GIS) to deliver the precursor gas into the sample chamber. Gas precursors are also used in gas-assisted etching (GAE) induced by ions, electrons, and laser beams.

[0006] Typically, it can be desirable to introduce different precursor gases during a deposition or GAE process. It is desirable to provide a gas injection system that is capable of handling multiple precursor gases, provides short switching times between precursors, is easy to set up, and requires minimal handling of chemicals. SUMMARY

[0007] The present disclosure relates to systems, methods, and apparatuses related to gas injection systems. In some embodiments, a gas injection system can include a housing configured to house a plurality of precursor reservoirs comprising one or more precursor materials, and a nozzle extending from the housing, the nozzle having a tip configured for insertion into a sample chamber of a material processing apparatus. The precursor reservoirs are fluidly connected to the nozzle to selectively deliver one or more precursor gases into the sample chamber.

[0008] In some embodiments, the housing includes a plurality of reservoir housings configured to receive precursor reservoirs. Each reservoir housing can include an integrated valve to fluidically connect a precursor reservoir disposed in the reservoir housing to the nozzle. In some embodiments, the housing can form a vacuum envelope around the plurality of precursor reservoirs. In some embodiments, each of the plurality of reservoir housings includes one or more temperature control elements configured to operate independently of one or more heating elements associated with other reservoir housings to maintain each of the plurality of precursor reservoirs at a temperature selected to sublimate a precursor gas in the precursor gas reservoir.

[0009] In some embodiments, the plurality of precursor reservoirs are fluidically connected in series to one or more delivery lines in fluid communication with the nozzle and the sample chamber. In some embodiments, the system can further include a plurality of three-way valves to fluidically connect the plurality of precursor reservoirs in series to the one or more delivery lines. In some embodiments, the one or more delivery lines are thermally controlled to prevent condensation of the precursor gas in the one or more delivery lines. In some embodiments, the one or more delivery lines are fluidically connected to one or more ejection capillaries disposed in the nozzle for delivering the precursor gas into the sample chamber. The nozzle can include a plurality of ejection capillaries for simultaneously ejecting a plurality of precursors into the sample chamber. In some embodiments, the nozzle is configured to be maintained under a thermal gradient along the length of the nozzle. The temperature can increase towards the tip of the nozzle. In some embodiments, the nozzle and the housing are configured to form a vacuum envelope around the precursor reservoirs and the one or more delivery lines.

[0010] The present disclosure also relates to a method for delivering a plurality of precursor gases into a sample chamber of a material processing apparatus. The method includes inserting a gas ejection system into the material processing apparatus. The gas ejection system can include a housing configured to house a plurality of precursor reservoirs including one or more precursor materials and a nozzle extending from the housing. The nozzle can have a tip configured for insertion into the sample chamber and the precursor reservoirs can be fluidically connected to the nozzle. The method further includes forming a vacuum in the housing around the plurality of precursor reservoirs, individually heating the plurality of gas precursor reservoirs to a temperature sufficient to generate one or more precursor gases from the one or more precursor materials, and selectively delivering the one or more precursor gases from the plurality of gas precursor reservoirs into the sample chamber.

[0011] In some embodiments, the method can further include heating the gas ejection system to a temperature sufficient to prevent condensation of the one or more precursor gases and maintaining the temperature. In some embodiments, the nozzle is configured to be maintained under a thermal gradient along the length of the nozzle.

[0012] In some embodiments, the housing includes a plurality of reservoir housings configured to receive a precursor reservoir. Each reservoir housing can include an integrated valve to fluidly connect a precursor reservoir disposed in the reservoir housing to the nozzle. In some embodiments, the plurality of precursor reservoirs are fluidly connected in series to one or more delivery lines in fluid communication with the nozzle and the sample chamber. The system can also include a plurality of three-way valves to sequentially fluidly connect the plurality of precursor reservoirs to the one or more delivery lines. In some embodiments, the one or more delivery lines are thermally maintained to prevent condensation of the precursor gas in the one or more delivery lines. The one or more delivery lines can be fluidly connected to one or more ejection capillaries disposed in the nozzle for delivering the precursor gas into the sample chamber. BRIEF DESCRIPTION OF DRAWINGS

[0013] Figure 1A is an exemplary embodiment of a gas injection system (GIS) of the present disclosure mounted on a main chamber of an instrument;

[0014] Figure 1B is an exemplary embodiment of a gas injection system of the present disclosure;

[0015] Figure 1C is an embodiment of the internal environment of a dual beam FIB / SEM instrument with a GIS inserted and gas release capillaries in close proximity to the sample processing region;

[0016] Figure 1D is an embodiment of the internal environment of a dual beam FIB / SEM instrument with the GIS retracted and gas release capillaries held at a safe distance from the sample processing region;

[0017] Figure 1E is an example of carbon material deposited by ion beam induced decomposition of volatile naphthalene delivered to the sample processing region by the GIS;

[0018] Figure 1F is a cross-sectional view of an example of platinum material deposited by ion beam and electron beam induced decomposition of an organometallic precursor delivered to the sample processing region by the GIS;

[0019] Figure 2 is an exemplary embodiment of a GIS body of a gas injection system of the present disclosure;

[0020] Figure 3A shows an exemplary reservoir housing with a reservoir inserted;

[0021] Figure 3B is a cross-sectional view of a reservoir suitable for use in a GIS system of the present disclosure;

[0022] Figure 4A and 4BAn exemplary embodiment of a tank suitable for use in the GIS system of the present disclosure is shown;

[0023] Figure 5A An exemplary schematic view of a tank conduit system is shown;

[0024] Figure 5B An exemplary tee valve suitable for use with the GIS system of the present disclosure is shown;

[0025] Figure 6A A cover of a GIS body having fittings for connecting gas tanks to gas lines is shown;

[0026] Figure 6B A location of a third tank having a precursor tank and a fourth tank having a precursor tank and a gas line is shown;

[0027] Figure 7A An internal view of a GIS body of the present disclosure is shown;

[0028] Figure 7B A tank housing mounted to a PCB having oversized holes is shown;

[0029] Figure 8A And Figure 8B An exemplary embodiment of a nozzle component is shown;

[0030] Figures 8C-8H A non-limiting example of a thermal management element of a nozzle is shown;

[0031] Figure 8I An exemplary nozzle alignment system is shown;

[0032] Figure 9 A cross-sectional view of an exemplary tank suitable for use in the GIS system of the present disclosure is shown;

[0033] Figure 10 An exemplary pneumatic actuation view of a tank suitable for use in the GIS system of the present disclosure is shown;

[0034] Figure 11 Is an exemplary flow chart of the process disclosed;

[0035] Figure 12 Is an exemplary flow chart of the controller state and logic flow representing in ready and running states;

[0036] Figure 13 Is an exemplary flow chart of the controller logic representing in set up;

[0037] Figure 14 Is an exemplary flow chart of the controller logic representing in service; and

[0038] Figure 15 is an exemplary flowchart representing a user operation logic flowchart.

[0039] While the above figures set forth presently disclosed embodiments, other embodiments can also be contemplated as indicated in the discussion. The present disclosure presents illustrative embodiments by way of representation and not by way of limitation. Those skilled in the art can devise many other modifications and embodiments that fall within the scope and spirit of the presently disclosed embodiments. DETAILED DESCRIPTION

[0040] It is the purpose of the gas injection system (GIS) of the present disclosure to enable the use of volatilizing agents and improve the efficiency of sample processing by delivering controlled amounts of reactive species for release in the vicinity of the sample processing area. According to some embodiments of the present disclosure, a chemical precursor or multiple chemical precursors can be delivered from a self-sealing precursor reservoir contained within an isolation envelope that surrounds all internal components of the apparatus. The flow rate and phase stability of these delivered precursors are managed by differential heating from the precursor reservoir housing, through the entire delivery path from the precursor source to the nozzle tip, by temperature control elements in thermal contact with the precursor reservoir housing. The arrangement of the precursor reservoir ports, valves, common delivery line, and evacuation ports support continuous high efficiency delivery, delivery line purging and cleaning, and continuous evacuation during idle periods.

[0041] In some embodiments, in the GIS of the present disclosure, multiple compatible precursor species can be loaded and maintained by independent reservoirs outside of the sample chamber of the instrument at a given time, but still in the internal vacuum portion of the GIS body. Thus, the GIS of the present disclosure is capable of processing samples with different precursor species using a single gas injector, eliminating the need for multiple GIS and eliminating the need for any adjustments upon precursor material change. It is made possible to change the spent precursor reservoir on the GIS of the present disclosure without breaking or entering the main sample chamber of the FIB, SEM, or similar instrument. In some embodiments, the GIS of the present disclosure provides continuous heating at the reservoir housing directly by a thermal shroud at all points throughout the precursor flow path. With this continuous heating combined with heat measurement at the location furthest from the heated element location on the precursor reservoir, the integration of heating control and feedback loops can prevent downstream condensation and / or solidification of the precursor within the GIS due to cooling of the precursor. Independent heating of each reservoir with chemical precursors can independently control the vapor pressure of each precursor, facilitating the regulation of flow rates. In some embodiments, the design of the GIS of the present disclosure incorporates differential heating of the injection nozzle, with heaters located near the tip and at the back of the delivery line. This differential heating across the heating elements creates a temperature gradient along the delivery line, preventing condensation of the precursor. The heating is beneficial for efficient removal of residual precursor from the line as all points of the delivery line are maintained at a temperature above the condensation temperature of the gas phase of the precursor material. In some embodiments, the GIS of the present disclosure has heating elements directly fixed to the precursor reservoirs of the GIS to provide direct heating to the area, making the heat transfer process more efficient and enabling fast feedback control.

[0042] In some embodiments, the GIS of the present disclosure is configured to prevent condensation of the precursor within the delivery line, and is thus suitable for precursors with low vapor pressure and precursors with significant vapor pressure, which can be in solid, liquid, or gas state under ambient temperature conditions. In some embodiments, the system is heatedly controlled using one or more temperature or thermal control elements, such as heaters, heat exchangers, heat spreaders, thermally conductive or insulating shrouds, and other similar temperature control devices, to maintain the system at a desired temperature to prevent condensation of the vapor within the system. In some embodiments, the GIS of the present disclosure has a single nozzle that does not have segments that stretch at different angles, and is thus capable of delivering multiple precursors without the need to change the GIS position or adjust the ion beam or electron beam that processes the sample.

[0043] In some embodiments, the GIS of the present disclosure does not require a carrier gas for precursor delivery. Precursor flow from the reservoir to the ejection capillary is facilitated by the vapor pressure of the heated precursor within the reservoir and supported by the temperature gradient created by continuous heating of the flow path and differential heating within the nozzle along the delivery line. In some embodiments, the GIS of the present disclosure is configured with a three-way valve at each precursor reservoir such that purging can be performed without additional valve actuation when the valve is closed at the precursor reservoir. The GIS of the present disclosure can also provide constant back pumping of the internal gas envelope at all times when no precursor is being ejected and constant back pumping of the inactive portion of the gas delivery envelope at all times while venting into a dedicated evacuation port or main chamber of the instrument. In some embodiments, the GIS of the present disclosure is based on a continuous delivery path with three-way valves in series, thereby completely eliminating manifolds and enabling fast switching between precursors to reduce cross contamination by constant back pumping and then completely eliminating cross contamination by a purge cycle with purging if necessary.

[0044] In some embodiments, the GIS of the present disclosure is configured such that all precursor species, typically in solid or liquid form, are contained within the vacuum envelope of the GIS body. In some embodiments, gaseous species that are chemically active or inert can also be ejected through gas reservoirs and / or from outside the GIS housing. The vacuum envelope serves as a safety enclosure for all precursors, providing isolation in the event of a leak from the precursor source and elements enclosed within the GIS body. In some embodiments, the precursors can be heated directly at the precursor reservoir, with differential heating along the gas line up to the end of the nozzle to control the flow rate of the precursor delivery without requiring any additional flow control devices. Continuous heating of the flow path and thermal gradient along the delivery line of the GIS of the present disclosure can prevent condensation and / or solidification of the precursors downstream of the precursor source.

[0045] In some embodiments, the GIS of the present disclosure is configured such that it can introduce precursor species into the sample processing space, in which the presence of a light beam irradiation provides conditions for processing with or without the presence of additional activator chemicals. In some embodiments, the GIS of the present disclosure can be used with multiple precursor gases and in a large number of focused light beam instruments.

[0046] In some embodiments, the GIS of the present disclosure provides continuous heating directly at the tank housing by a thermal shroud at all points throughout the precursor flow path. The integration of heating control and feedback loops, combined with heat measurement at the point furthest from the heating element location on the precursor tank, prevents condensation and / or solidification of the precursor downstream within the GIS due to precursor cooling. Independent heating of each tank using the chemical precursors enables independent control of the vapor phase of each precursor, which helps to regulate flow rates. The design of the GIS of the present disclosure can incorporate differential heating of the nozzle, with heaters located near the tip and at the back of the delivery line. The differential heating across these heating elements creates a temperature gradient along the delivery line or tube, preventing condensation of the precursors. In some embodiments, all points of the delivery line are maintained at a temperature higher than any of the precursor tanks, and the heating facilitates efficient removal of residual precursors from within the tube. In some embodiments, the GIS of the present disclosure has heating elements directly fixed to the precursor tanks or tank housing of the GIS to provide direct heating to the area, making the heat transfer process more efficient and enabling fast feedback control. In some embodiments, the present design prevents condensation of the precursors within the delivery line, and is therefore suitable for precursors with low and significant vapor pressures, which can be solid, liquid, or gas at ambient temperature conditions.

[0047] In some embodiments, the GIS of the present disclosure does not require a carrier gas for precursor delivery. Precursor flow from the tank to the delivery line is facilitated by the vapor pressure of the precursor material within the heated tank, and is supported by continuous heating of the flow path and a temperature gradient along the delivery line and nozzle created by differential heating. The precursor material can be in solid or liquid form, or in gas form. In some embodiments, the GIS of the present disclosure is configured with a three-way valve at each precursor tank, such that when the valve is closed at the precursor tank, purging can be performed without additional valve actuation. The GIS of the present disclosure can also provide constant back pumping of the internal gas envelope at all times when no precursors are being ejected, and constant back pumping of the inactive portion of the gas delivery envelope at all times, while venting into a dedicated evacuation port or main chamber of the instrument. The GIS of the present design is based on a continuous delivery path with three-way valves in a serial arrangement, eliminating manifolds entirely and enabling fast switching between precursors to reduce cross-contamination by constant back pumping, and then completely eliminating cross-contamination by a purge cycle if necessary.

[0048] All precursor types (typically in solid or liquid form) of the GIS disclosed herein are contained within a vacuum enclosure of the GIS body. This vacuum enclosure serves as a protective housing for all contained precursors, providing isolation in the event of a leak at the precursor source. Furthermore, the precursors are thermally controlled directly at the precursor storage tank, with differential heating along the gas pipeline to the nozzle tip to control the precursor delivery rate without any additional flow control devices. Continuous heating of the flow path and the thermal gradient along the delivery pipeline of the GIS of this disclosure prevent condensation and / or solidification of the precursors downstream of the precursor source.

[0049] In some embodiments, the gas-assisted process may include local activation through a spontaneous reaction between precursors and activating chemicals on the sample surface, even after beam irradiation has ceased; however, the GIS disclosed herein is not limited to such methods of depositing or removing material in any configuration. Precursor species may be introduced into the sample processing space, where the presence of beam irradiation provides the conditions for processing regardless of the presence of additional activating chemicals. In some embodiments, organometallic chemicals for ion beam deposition, such as methylated and / or ethylated metals (e.g., hexamethyldistin), may be used to produce very low resistivity deposits. In some embodiments, the GIS of this disclosure may utilize, but is not limited to, their individual use. Likewise, the GIS disclosed herein will be used in a wide range of focused ion, electron, and laser beam instruments.

[0050] Figure 1 illustrates an exemplary embodiment of the GIS system 10. In some embodiments, such as Figure 1A As shown, in the GIS of this disclosure, multiple chemically compatible precursor species are loaded into the GIS body 14 at a given time via independent tanks and kept outside the sample chamber 12 of the material handling instrument (e.g., scanning electron microscope (SEM)), focused ion beam (FIB) instrument, dual-beam FIB / SEM, laser beam-based instrument, or similar instrument), but still within the internal vacuum of the GIS body 14. Therefore, the GIS of this disclosure can process samples with different precursor species using a single gas injector that can be mounted on the sample chamber 12, thereby eliminating the need for multiple GIS and eliminating the need for any adjustments when precursor materials are changed. This allows for the replacement of depleted precursor tanks on the GIS of this disclosure without disrupting the vacuum or otherwise interfering with the environment in the main sample chamber of the FIB, SEM, or similar instrument. Figure 1A As shown, the GIS system 10 may also include an electrical connection 16 to the controller and a pumping line 18.

[0051] The gas injection system disclosed herein (e.g., such as...) Figure 1B (As shown) is a complete multi-chemical GIS. Figure 1BThe GIS system 10 shown in FIG. 1 includes an ambient atmospheric portion 52 and an instrument chamber portion 54. For use, the device is installed on an instrument having the instrument chamber portion 54 housed within the sample chamber 12, and the portion 52 remains outside the instrument, as shown in FIG. 2. Figure 1A

[0052] The GIS system 10 also includes a GIS body 14, which is configured to house precursor reservoirs. In some embodiments, the GIS body 14 can have the shape of a cube (aka “cuboid”), but can have other shapes as well. The GIS body houses the internal components of the system, including a plurality of precursor reservoirs. Within the sealed GIS body, chemical precursors are contained for safety and performance purposes. The sealing of the GIS body provides failsafe protection in the event of an accidental leak from any of the internal reservoirs or conduit systems. Since the GIS body is also maintained under vacuum pressure, heat transfer from the reservoirs and conduit systems is well isolated for reliable temperature control. This vacuum insulation can ensure that the GIS body is maintained at or near room temperature while heating the internal components. In some embodiments, the GIS body 14 is maintained under vacuum to correspond to the vacuum of the sample chamber 12. In some embodiments, the GIS body 14 is maintained under vacuum by a dedicated pump through a pumping line 18. Since the GIS housing is sealed from the sample chamber 12, the precursor reservoirs can be replaced, if necessary, without breaking the vacuum or disturbing the internal environment of the sample chamber 12.

[0053] In some embodiments, the GIS of the present disclosure possesses a single nozzle 20 to deliver multiple precursors from the GIS body 14. This can enable delivery of various precursors without the need to change the GIS position or without the need to make adjustments to the ion beam or electron beam from the ion beam source 22 or electron beam source 24 that processes the sample, as shown in FIG. 3. Figure 1C and 1D Directing precursors from a single nozzle can eliminate the need to change the nozzle 20 tip position in order to direct different chemicals to the ion beam from the ion beam source 22 or the electron beam from the electron beam source 24 and the substrate material located on the sample processing region 26. Referring back to FIG. 1, the GIS system 10 can also include an X-direction nozzle adjustment knob 56, a Y-direction nozzle adjustment knob 58, which are capable of adjusting the position of the nozzle relative to the ion beam or electron beam. Figure 1F

[0054] During operation, the nozzle 20 of the GIS system 10 can be inserted into the sample chamber 12, and the GIS system 10 can be secured in place using a mounting bracket 64. The nozzle 20 can be moved from a retracted position, as shown in FIG. 4, to an inserted position, as shown in FIG. 5, which is proximate to the sample work area. The vacuum bellows 62 facilitate this movement while maintaining the integrity of the internal vacuum environment. Figure 1D Figure 1C ​​​​

[0055] Figure 1E An example of carbon material 30 deposited by ion beam induced decomposition of a volatile naphthalene delivered by a GIS to a sample processing area (substrate 32) is shown. Figure 1F A cross-sectional view of an example of platinum material 40 deposited by an ion beam and platinum material 42 deposited by electron beam induced decomposition of an organometallic precursor delivered by a GIS to a sample processing area is shown. Once inserted into the apparatus, the GIS delivers the precursor to the sample work area within the sample chamber for processing using a particle beam. Precursor delivery operations including valve actuation, precursor selection, and GIS insertion are all managed by the user through a controller and PC software.

[0056] As noted above, the GIS body 14 is maintained under vacuum during GIS system operation. The GIS body can be pumped to vacuum pressure in a variety of ways. In some embodiments, a nozzle that can reside in the sample chamber can be used. In some embodiments, the nozzle used to deliver the precursor can also be used as an opening to pump the internal plumbing and volume of the GIS to the vacuum of the sample chamber when no active deposition precursor is present. In some embodiments, one or more ports can be positioned on the GIS body where a line can be run to an external pump or vacuum chamber of an instrument.

[0057] With reference to Figure 2 The GIS body 14 includes ports 80, 82 to which vacuum lines can be attached. The use or non-use of these ports can be configured in a variety of ways depending on whether or not continuous back pumping of the internal gas plumbing is required and which of the two pumping methods is selected. Briefly, if the GIS body 14 can be pumped into the main chamber of the SEM / FIB instrument and the internal gas plumbing is not back pumped with all of the ejection valves closed, then no vacuum ports will be used at the bottom of the GIS body. If the GIS body is pumped into the main chamber of the instrument and the internal gas plumbing is back pumped with all of the ejection valves closed, then one vacuum port will be used at the bottom of the GIS body. If the GIS body is pumped by a separate vacuum line and the internal gas plumbing is not back pumped with all of the ejection valves closed, then one vacuum port will be used at the bottom of the GIS body. Finally, if the GIS body is pumped by a separate vacuum line and the internal gas plumbing is back pumped, then two vacuum ports will be used at the bottom of the GIS body.

[0058] As Figure 2 Further shown, a gas cylinder 84 is disposed on the GIS body 14 that can receive compressed gas for extending and retracting the nozzle at adjustable speeds.

[0059] Linear movement of the nozzle can be used Figure 2The two air cylinder actuators shown are used to control. In some embodiments, the air spring cylinders provide just enough force to overcome atmospheric pressure acting on the device. This means that when the device is in the home position or the compressed air line is broken, the device will fully retract, protecting itself and other components from impact. During the point of operation, the cylinders control the extension and retraction of the nozzle at an adjustable speed. When the GIS is used for sample processing, the nozzle will be extended from a retracted position in the instrument chamber to the sample work area by the cylinder. After the GIS processing is complete, the GIS can be retracted by the same cylinder to clear the work area around the sample and protect the instrument.

[0060] The GIS body can further include an insertion linear guide 86 and a retraction air spring 88 to assist in the movement of the nozzle or GIS housing relative to the instrument. The GIS body 14 also includes a communication and power connection port 89 to provide connectivity to a printed circuit board (PCB) that enables the electrical components of the GIS system 10 to operate. In some embodiments, fine tuning of the insertion depth can be provided by adjusting a set screw 87 on the back of the air spring 88. In some embodiments, the air spring can only compress when its shaft is fully inserted and a hard stop is engaged. The position of the GIS body relative to the air spring shaft hard stop position can be adjusted by the set screw 87.

[0061] Reference is made to Figure 3A and 3B , a reservoir of chemical precursors is housed in a compact array of ports. In some embodiments, a plurality of reservoir ports 90a, 90b, 90c, 90d can be arranged on the base of the GIS body. Each port 90a, 90b, 90c, 90d can include a reservoir housing 92a, 92b, 92c, or 92d, respectively, configured to receive a precursor reservoir 94. One or more temperature control devices 95 can be provided to vaporize the precursors. In some embodiments, the temperature control device 95 can be a resistive heater. In some embodiments, the temperature control device 95 can be a thermoelectric heat transfer element, such as a Peltier or other device. In some embodiments, the temperature control device can be located at the valve of each reservoir port. The system also includes one or more precursor flow and pumping ports 97 that fluidically connect the ejection nozzle, located within the sample chamber, to the precursor reservoirs to enable the delivery of precursor gas into the sample chamber. The reservoir ports 90a-90d are designed to facilitate reservoir replacement.

[0062] Figure 3B and 4A -4B provides an exemplary embodiment of a self-sealing reservoir. In some embodiments, such a reservoir assembly can be used for non-corrosive solid and liquid precursors. However, it should be noted that reservoirs with gaseous substances can also be used. As Figure 3BAs shown, the precursor tank includes a tank body 105, a tank base 108, and a precursor internal volume 110, which is designed to contain precursor material. An O-ring 107 may be provided to form a seal around the tank base 108. In some embodiments, the tank is delivered to the user along with liquid or solid precursor material preloaded into the internal volume 110. The liquid or solid phase of the precursor material can be retained within the internal volume 110 by a permeable barrier, which allows for the gaseous phase transfer of the precursor. For example, a filter media compatible with the precursor material can be used as a permeable barrier.

[0063] In some embodiments, the storage tank 94 further includes a spring 100 held by a retaining bushing 101. When the spring 100 is compressed, it is configured to apply pressure to the plunger 102, which in turn compresses the inner O-ring 106, effectively sealing the precursor in the inner volume 110 and the gas phase within the storage tank. When the storage tank is inserted into the storage tank housing, the plunger 102 and... Figure 7B The tank valve actuator is engaged, yet the tank remains sealed by the plunger 102 and the compressed O-ring 106. When the tank is secured to the tank housing by one or more retaining screws, the threaded action pushes the tank further into the tank housing. The tank valve actuator can be configured to act on the plunger 102 against the force of the spring 100, moving the plunger 102 with the internal O-ring away from the tank body. Simultaneously, the O-ring contacts the bottom of the tank housing and is compressed by the action of securing the tank to the tank housing, thus forming a seal. As the internal valve opens by the reverse movement of the plunger and a seal is formed between the tank and the housing by the compressed O-ring, the gaseous phase of the precursor material can be released into the sealed volume and reach the normally closed inlet of the three-way valve 112. The temperature of the tank can be set to the desired value by the action of a heater or thermoelectric heat transfer device (e.g., arranged on the tank body), thereby generating the desired pressure of the gaseous phase of the precursor material. A control signal can be supplied to a flow control device, such as a three-way valve 112, to open it and release the gaseous phase of the precursor material into the delivery line. The delivery line, which is fluidly connected to a capillary at the nozzle tip via a gas delivery tube, delivers the gaseous phase of the precursor released from the capillary to the sample chamber.

[0064] refer to Figure 5A This describes the configuration of the tank piping system.

[0065] A plurality of valves 112a, 112b, 112c, 112d can be provided to fluidly connect precursor reservoirs disposed in reservoir housing ports 90a, 90b, 90c, and 90d to one or more delivery gas lines 111. The delivery gas lines 111 fluidly connect the reservoir ports to gas delivery lines to deliver precursor gas to the nozzle and then into the sample chamber, and also allow for venting or purging of precursor gas from the lines. By switching a series of valves 112a, 112b, 112c, 112d, the gas phase of a precursor from any one of the reservoirs can be flowed into the delivery gas line 111 and downstream to the nozzle. In some embodiments, the valves 112a, 112b, 112c, 112d are three-way valves. The actuation of the three-way valves can ensure that there is either (1) flow of precursor gas in the downstream delivery path toward the nozzle isolated from everything upstream or (2) full delivery line back-pumping and / or purging with a dedicated purge gas due to reverse pumping and / or purging of the common delivery line through a dedicated port on the GIS body or one of the reservoir ports. In some embodiments, the delivery gas lines 111 are maintained at a temperature that prevents condensation of the precursor in the delivery gas lines 111. In some embodiments, at least some portions of the delivery gas lines 111 include a thermally conductive sheath 113 that can be maintained at a desired temperature that surrounds the delivery gas lines 111. Additionally or alternatively, one or more other heating or insulating elements can be employed to maintain a desired temperature of the delivery gas lines 111.

[0066] Referring to Figure 5B In some embodiments, a suitable three-way valve 112 has 3 ports: a normally closed (NC) port 115; a switching port 116; and a normally open (NO) port. When the three-way valve is in its initial state, un-actuated, the NC port 115 is sealed while the NO port 117 is fluidly connected to the switching port 116. When the valve is actuated, the NO port 117 is sealed while the NC port is fluidly connected to the switching port 116, allowing gas phase precursor to flow in the downstream delivery path to the ejection capillary. When the valve is de-actuated, it returns to the initial state where the NC port is sealed while the switching port is fluidly connected to the NO port in the upstream direction. Thus, in operation, a reservoir can be fluidly connected to the NC port, a delivery line downstream of the instrument to deliver precursor can be connected to the switching port, and an upstream delivery line for venting / purging can be connected to the NO port. In this way, when the valve is un-actuated, the common delivery gas line 111 can be back-pumped, purged with a compressed gas, or gaseous precursor can be delivered to the instrument from outside the GIS body. Furthermore, the precursor reservoirs can be connected to or isolated from the delivery line by controlling the state of their respective three-way valves to deliver precursor gas to the instrument or to purge.

[0067] Referring to Figure 6A and 6BIn some embodiments, to clean the delivery gas line 111 when switching precursor materials or as part of preventative maintenance, an additional port 120 is provided, for example at the back cover 122 of the GIS body, to be connected to an external gas source or exhaust pump. Within the GIS body, the port 120 is fluidly connected to a gas reservoir 123, which can be installed within one of the gas reservoir housing ports. In some embodiments, the gas reservoir 123 can be connected to evacuate or purge the line through the last gas reservoir port. In that case, the pumping provided through the port 120 first evacuates the gas reservoir and gas reservoir housing ports. When the valve 112d is opened, the vacuum within the gas reservoir becomes fluidly connected and evacuates the gas line connected fourth to third, third to second, etc., and then pumps or purges the entire gas delivery, such as the downstream of the ejection capillary. Alternatively, a gas can be supplied through the port 120 into the gas reservoir 123. When the corresponding valve 112 is opened, the gas can purge the gas line installed downstream of the gas reservoir port of the gas reservoir 123. These reverse pumping and molecular scrubbing (purging) cleaning methods are fast and reliable. They can save a significant amount of time and are more effective compared to the traditional cleaning method of just heating and opening the nozzle. In some embodiments, the port 120 can be used to introduce another gas precursor or reaction gas into the system during device operation.

[0068] When all valves 112a-112d are switched to closed, reverse pumping for the common delivery gas line 111 is provided through a dedicated port 80 on the GIS body, which is fluidly connected to the exhaust / purge fitting in Figure 5A As part of a purging cycle, compressed gas can be supplied through the same port to purge residual precursors from within the common delivery gas line 111. The series connection of the normally open ports of the valves 112a-l12d forms a continuous path to evacuate or purge-clean the common delivery gas line 111 when switching precursor materials or as part of preventative maintenance.

[0069] It should be noted that while the precursor material is typically a vaporizable solid or liquid, in some embodiments, chemically active or inert gaseous substances may also be injected via gas tanks and / or from outside the GIS housing. It should also be noted that in some embodiments, reverse pumping or purging of the entire gas pipeline can also be accomplished via external port 80, which may be fluidly connected to the "exhaust / purge" fitting of the gas delivery pipeline 111. Alternatively, the exhaust / pump port may be connected to the instrument's main chamber maintained at vacuum pressure, or other vacuum volume. This pumping will occur when all valves 112a, 112b, 112c, and 112d are closed. In some embodiments, reverse purging of the entire gas delivery system (including the piping system and gas pipelines) can be accomplished by supplying an inert or chemically inert gas to the exhaust / purge fitting when the exhaust / purge fitting is connected to the external pumping port 80.

[0070] In some embodiments, the heating process, which controls the gas phase pressure of the precursor, is performed by a device located at, for example, Figure 3A Temperature control is implemented at the valve at each tank port, as shown. In some embodiments, the temperature control device is a resistance heater or a thermoelectric heat transfer element. Furthermore, the system is designed so that the vaporized precursor does not condense in the gas line upon delivery to the sample chamber. Temperature is measured by a sensor, which can be mounted on each tank housing 92 at the point furthest from the heater (i.e., the top), such as... Figure 7A As shown. By doing so, the entire precursor tank is ensured to be heated to at least the measured temperature, which can be positioned above the sublimation point of the precursor to provide the required vapor phase pressure. This, combined with the high vacuum within the GIS body, helps ensure stable vaporization and prevents condensation at or near the valves or on the back of each tank. In addition to utilizing the high vacuum within the GIS body to eliminate convective heat transfer, the gas delivery lines 111 connecting the tanks can be made of resistant plastic, wrapped with a thermally conductive shielding layer to mitigate heat loss through radiative heat transfer and reduce the risk of condensation in the lines. Naturally, chemicals with the lowest vaporization temperatures can be placed furthest upstream from the nozzle, as they may have a longer path to the nozzle. Reference Figure 7B Furthermore, PCBs can be provided for mounting on platforms supporting the tank shell to minimize heat transfer. Through-plate channels can be large enough to prevent heat loss from heated components due to conduction, and the plate is layered with a non-thermally conductive polymer (e.g., PEEK polymer). Mechanical mounting of the tank shell can also be achieved using insulating supports with low thermal conductivity.

[0071] Figure 7B A tank valve actuator 132a is further shown, disposed within the tank shell 92a and in communication with a three-way valve 112a. In operation, the tank valve actuator facilitates fluid connection between the tank's precursor reservoir and the three-way valve.

[0072] Referring to Figures 8A-8I , components of the nozzle 20 are described. As described above, the nozzle 20 is connected to the GIS body to deliver precursor gases to the instrument. In some embodiments, the nozzle 20 is designed to maintain a temperature necessary to prevent condensation of vapor within the nozzle. In some embodiments, the nozzle can include a set of metallic tubes. Referring to Figure 8A , the outer tube 131 houses an inner gas line 130, which is connected to the delivery gas line 111 to deliver precursor gases to the nozzle. In some embodiments, the inner gas line 130 is a stainless steel tube. One or more gas capillaries 136 can be provided at the end of the nozzle, in communication with the inner gas line 130 to deliver precursor gases into the sample chamber. In some embodiments, a single capillary can be used if the precursor gases can be mixed and delivered together, while multiple capillaries can be used if separate delivery of precursor gases is desired. It should also be noted that, as described above, multiple inner gas lines 130 can be employed.

[0073] In some embodiments, the temperature of the inner gas line can be maintained above the vaporization temperature of the gas phase of the precursor in the line, so that vapor inside the gas line does not condense. If multiple delivery lines are used, each line can be heat controlled, but can be maintained at different temperatures depending on the nature of the precursor gases delivered through each gas line. In some embodiments, the inner gas line 130 can be surrounded by a thermally conductive sheath 133 to maintain the temperature of the inner gas line 130. The space between the inner gas line 130 / thermally conductive sheath 133 and the outer tube 131 can define a chamber, which can be under vacuum to remove convective heat transfer from the inner gas line 130. In some embodiments, additional insulation or heating can be added around the inner gas line 130.

[0074] Towards the end of the nozzle, the thermally conductive sheath 133 transitions to an external heat sink 135 under a coupler 137, as Figure 8BThe outer heat sink can be made of highly polished gold plated copper in some embodiments. In addition, the nozzle end of the heat conductive sheath can be equipped with one or more heaters 134. For example, a first heater 134 can be located near the upstream end of the outer tube and can be made of thin film resistive material. In some embodiments, the heating element can be a heater, heat exchanger, heat conductive sheath, or heat sink. Another heater 134 can be located downstream of the outer tube. In some embodiments, the difference in heat dissipation of the nozzle heater and the heater for the reservoir housing can result in a temperature difference of several degrees, where the area of the conductive cap end is typically the hottest throughout the ejector. A slight temperature gradient, typically about 3 to 5 degrees Celsius, facilitates the emission of thermal radiation from the end of the heat conductive outer heat sink, thereby heating the ejection capillary and facilitating the stable flow of the gas phase without the risk of condensation at the nozzle exit. The high polish surface of the heat sink cap can also minimize radiative heat transfer to the chamber environment and the sample.

[0075] Further non-limiting examples of thermal management elements of the nozzle are provided in Figures 8C-8E . Figure 8C The tip of the heat conductive sheath protruding from the lower coupler is shown (the outer heat sink with gas delivery line and ejection capillary are not shown). Figure 8D The heat conductive sheath / heat sink is shown. The temperature control element or thermal control element (e.g., heater 134) is wrapped around the gas line. Figure 8E The gas delivery line with sheath is shown. An example of a heater positioned on the heat conductive sheath within the nozzle is shown in Figures 8F-8H . Figure 8F The heater near the sheath capillary end is shown. The black substance is a heat shrink tube covering the actual heater below. This end is inserted under the outer heat sink. Figure 8G The sheath back end located on top of the gas delivery line, near the gas line connection point is shown. The back temperature control element (thin film resistor) is installed. Figure 8H The sheath back end with temperature sensor attached is shown.

[0076] Reference is made to Figure 8IThe nozzle can be provided with an alignment block 140 for adjusting the position of the nozzle within the sample chamber as described above. The alignment block can be located on the outer tube 131, and the inner gas line 130 can pass through the alignment block 140. The inner gas line 130 can be connected to the common gas line at a gas line connection 138. The alignment block 140 can include a set screw 142 for adjusting the x-direction and a set screw 144 for adjusting the y-direction of the nozzle. The alignment block can also include an alignment spring 146 that biases the inner tube 138 towards the center of the alignment block. The extension depth can be fine-tuned by adjusting the respective set screws, and the overall movement has a hard stop on a linear slide bearing. Control over the lateral position of the nozzle is controlled by knobs 56 and 58 mounted on the housing. In some embodiments, the knobs drive a rod into the alignment block 140 or the stainless steel inner gas tube to overcome the resistance of the alignment spring 146 to move it. The rods 142, 144 interact with the inner tube at an upstream point before the O-ring connection portion of the stainless steel inner gas tube. The force is applied away from the O-ring fulcrum point, resulting in a significant movement for a small change in knob position. All directional alignments have a typical 5-micron repeatability. Figure 8C An upper coupler 148 of the nozzle is also shown.

[0077] Figure 9 and 10 Another embodiment of a tank suitable for use in a GIS system of the present disclosure is shown. In some embodiments, this design can be associated with a corrosive precursor, such as liquid bromine or solid iodine. Referring to Figure 9 A tank for a corrosive precursor is shown in a tank housing. This tank 150 can have a similar internal structure as the tank for a non-corrosive precursor shown in Figure 3B and Figures 4A-4B As shown in Figure 9 The liquid or solid precursor material can be placed in the internal volume of the precursor reservoir 152 and can be held there by a gas permeable membrane. The precursor can be sealed in the internal volume of the precursor reservoir 152 of the tank by a plunger O-ring 154, which is pushed against the tank body 156 by a compressed internal spring 158.

[0078] The front of the corrosive precursor tank can include a spout that is inserted into a receiving channel within the tank housing. A gas-tight sliding seal is formed between the spout and the channel in the tank housing, allowing the tank to move along the channel. The seal can be formed by an elastomeric X-O-ring 160 that is inserted into the channel within the tank housing and compressed between the spout and the channel within the tank seal.

[0079] Referring to Figure 10, the corrosive reservoir 150 can be positioned within the reservoir housing 168 such that its plunger 162 contacts the valve actuator pin 163. The force of the reservoir body 156 pushing against the valve actuator pin is resisted by the force of one or more compressed reservoir retraction springs 164 and the reservoir’s internal spring. As shown in Figure 10 The release of precursor from the reservoir 150 is accomplished by the action of compressed air being injected into the expansion bellows 172 via the compressed air inlet 170. The build-up of internal pressure within the bellows causes the bellows to expand in the axial direction of the reservoir. The expanding bellows can exert a force against the reservoir base 166, thereby overcoming the resistance of the reservoir retraction springs and the reservoir’s internal spring, and causing the entire reservoir to move further axially into the reservoir housing 168. This axial movement can cause the valve actuator pin to cause the plunger to move away from the base of the reservoir body. This movement can cause the pressure release of the plunger O-ring and the opening of the fluid connection between the internal volume of the reservoir and the reservoir housing, thereby releasing the precursor stream from the reservoir to the reservoir housing and further into the gas delivery line.

[0080] Referring to Figure 11 , an exemplary process flow diagram is presented. In step 180, one or more precursor reservoirs are loaded into the gas injection system. The precursor reservoirs are inserted into the reservoir housing of the GIS body. In step 182, a vacuum is created in the GIS body to create a vacuum envelope around the reservoirs. Next, the reservoirs can be individually heated to vaporize the precursor material. Additionally, the system is heated to prevent condensation of the precursor gases in the system. In step 184, the selected one or more valves are opened to allow the precursor gas to flow from the selected reservoirs into the delivery line and into the nozzle and continue into the sample chamber. In step 186, the precursor gas or mixture of precursor gases can be selectively delivered into the sample chamber by connecting or disconnecting various reservoirs with the delivery line. As the precursor gas is delivered into the sample chamber, the vacuum and temperature in the system remain constant. As described above, if necessary, the precursor reservoirs can be switched by breaking the vacuum in the GIS body but not the vacuum in the instrument. In step 188, the flow of precursor gas is shut off and the system can be purged in step 190.

[0081] The present disclosure includes various embodiments of the above methods, systems, and components as follows: In some embodiments, a multi-precursor gas injector mounted on a FIB, SEM, or other instrument has its internal volume evacuated directly into the instrument's chamber through a dedicated evacuation port or evacuation opening, thereby forming a vacuum jacket around all internal elements of the gas injector. In some embodiments, the reservoirs with chemical precursors are completely enclosed within the vacuum jacket. In some embodiments, the vacuum jacket around the reservoirs with precursors provides an auxiliary container for the chemicals sealed within the reservoirs. In some embodiments, the vacuum jacket around the reservoirs with precursors acts as a thermal barrier to prevent heat transfer between the reservoirs and between each reservoir and other elements of the injector. In some embodiments, the reservoirs with chemical precursors contain integrated valves that remain normally closed during shipping and installation of the reservoirs. The valves can be opened when the reservoirs are installed within the gas injector. In some embodiments, after installation of the reservoirs, the integrated valves can be maintained in the open position, with the flow of precursors from the reservoirs controlled by additional shut-off valves elsewhere in the reservoir housings or elsewhere. In some embodiments, the integrated valves within the reservoirs are used to control the flow of precursors out of the reservoirs by mechanically actuating the position of the reservoirs within their housings. In some embodiments, the valves integrated within the reservoirs are used to control the flow of precursors from the reservoirs by mechanically actuating the valves, while the reservoirs remain in a fixed position within their housings. In some embodiments, the actuation of the valve position can be pneumatic, electromagnetic, electromechanical, piezoelectric, or other means. In some embodiments, the temperatures of the reservoirs, their housings, elements of the flow path, and other elements of the injector are maintained at temperatures above, at, or below ambient as needed to control the pressure of the precursors delivered from the reservoirs and to prevent condensation of the precursors on elements of the delivery system. In some embodiments, temperatures above ambient can be maintained by heaters in close mechanical and thermal contact with the reservoirs or their housings. In some embodiments, temperatures above, at, and below ambient can be maintained by heat transfer devices such as Peltier elements, heat exchangers, or other thermal or temperature control / transmission elements in close mechanical and thermal contact with the reservoirs or their housings. In some embodiments, excess heat generated by the active heat transfer devices is removed by close mechanical and thermal contact with the outer housing of the jacket, convective cooling, or by heat exchangers through which a refrigerant flows. In some embodiments, inserts within the heat exchanger channels can be added to force the refrigerant to flow along the channel walls and to mix the refrigerant during the flow to improve the heat transfer efficiency within the heat exchanger. In some embodiments, temperatures below ambient can be maintained by heat removal devices in close mechanical and thermal contact with the reservoirs or their housings, such as by heat exchangers through which a refrigerant flows. In some embodiments, a thermal feedback loop independently controls the temperature of all or each of the reservoirs with chemical precursors within the same vacuum jacket. In some embodiments, the pressure of the precursors in the reservoirs is regulated by controlling the temperature of the reservoirs and their respective housings.In some embodiments, chemical precursors are transported between reservoirs and to the ejection capillary through tubing systems that resist attack by the precursors. In some embodiments, the tubing systems that deliver the chemicals are enclosed in a thermal sheath that has conditions suitable for flowing the precursors without condensation, decomposition, or other adverse effects on the transported materials. In some embodiments, the sheath can be rigid, for example made of aluminum, copper, or other metals with suitable thermal conductivity. In some embodiments, the sheath can be flexible or semi-flexible, for example made of copper or aluminum foil, wire braid, mesh, tape, or thermally conductive rubber or flexible composite without a metal core. In some embodiments, the temperature and thermal gradient on the sheath can be defined by the thermal conductivity of the sheath material physically connected to the thermally controlled reservoirs or housing. In some embodiments, the temperature and thermal gradient of the sheath can be controlled by independent heaters mounted on the sheath along its length or at specific locations needed to create the thermal gradient. The heaters of the sheath can operate at fixed, predetermined temperatures or can employ feedback loops to control the temperature of the sheath. In some embodiments, the temperature and thermal gradient of the sheath can be created and controlled by passing an electric current through the sheath. In some embodiments, compatible chemical precursors from different reservoirs are delivered to the instrument through a single ejection capillary. In some embodiments, the connection of the compatible chemical precursors to the single ejection capillary within a vacuum envelope is in series with a three-way ejection valve on each precursor housing, or through a parallel manifold. In some embodiments, in a manifold connection, the precursor housing can have a two-way on-off valve that interrupts the flow of the precursor. In some embodiments, in a manifold connection, each precursor flow can be interrupted by a three-way valve. In some embodiments, when the flow of a precursor gas is interrupted, a purge gas can be ejected into the manifold or gas ejection capillary to remove residual precursor. In some embodiments, the valves of the manifold and series connections can be operated sequentially, thereby ejection a plurality of precursors or mixtures thereof through the capillary. In some embodiments, more than one capillary can be employed to simultaneously eject incompatible precursors. In some embodiments, the ejection capillary can release the precursors directly into a chamber of the instrument, or a gas concentrator can create a virtual processing chamber near the sample surface. In some embodiments, the chemical precursors that are ejected into the instrument through the delivery capillary can interact with a sample material maintained at a temperature above, equal to, or below ambient temperature. In some embodiments, the temperature of the sample can be maintained above ambient temperature by an electrical resistance heater or heat transfer device. The heat transfer device can be passive (e.g. a heat exchanger) or active (e.g. a Peltier or similar element). In some embodiments, excess heat is removed from the sample or Peltier or other active heat transfer element that controls the temperature of the sample by flowing a heat transfer fluid or other medium through internal channels of a heat exchanger in close mechanical and thermal contact with the sample or heat transfer element.In some embodiments, the heat exchanger channel may include an insert that forces the refrigerant to flow along the channel wall and mixes the refrigerant during the flow.

[0082] The following descriptions and procedures are presented as non-limiting examples of the methods, systems, and apparatus of this disclosure.

[0083] The examples presented to aid in understanding this disclosure should not be construed as limiting the scope of this disclosure in any way as defined in the following claims. The following embodiments are provided to provide a description of one embodiment of the complete disclosure and how to make and use the disclosure to those skilled in the art, and are not intended to limit the scope of what the inventors consider their invention, nor are they intended to represent all or only the experiments conducted. Efforts have been made to ensure the accuracy of the figures used (e.g., quantities, temperatures, etc.), but some experimental errors and biases should be taken into account.

[0084] Example: Description of controller states

[0085] Figures 12-15 A non-limiting embodiment presents a flowchart of the system state. Figure 12 This indicates the controller state and logic flow when it is in a ready or running state. Figure 13 This indicates that the controller logic is in the current state. Figure 14 This represents the controller logic that is in a service state. Figure 15 This represents a flowchart illustrating the user operation logic.

[0086] like Figure 15 As shown in the exemplary state flowchart, upon startup, the system is in the "Off" state, the GUIPC connects to the controller, and the executable software starts. If the key is in the "Setup" position when the system is powered on, the system will remain in the default "Idle" state indefinitely until the key is turned to the "Run" position. The system can then be in a variable "Idle" state. Once the system is in "Setup" mode, if the system moves to "Service" mode, the "Enable" state button on the back of the controller can be pressed. In the next step, the system can be in the "Service" state. If the key is switched from the "Setup" state to the "Run" state, the system will enter the "Idle" state. Pressing the "Enable" button moves the system into the "Enable" state. If all readbacks are within tolerance and the interlocks are inactive for 10 seconds, the system enters the "Ready" state. If one or more "Jet / Off" buttons are turned on, the system enters the "Run" state, allowing sample processing to begin.

[0087] There are various system changes that affect the system state.

[0088] 1. Uploading executable software should reset the controller and put it into an "idle" state.

[0089] 2. Connection and disconnection of the GUI PC from the controller shall not cause the controller to reset nor shall it affect its operation in any way.

[0090] 3. "Off" state - power off, all injection valves closed, GIS inserted gas valve closed, GIS retracted. The controller can only be switched from the "Off" state to the "Idle" state. The "Off" state is entered from any other state by turning off the power to the controller.

[0091] 4. Regardless of the position of any button, key or switch, power up enters the "Idle" state. In the "Idle" state, all injection valves are closed, the GIS is retracted, the heater and Peltier are disabled, the back read is "enabled", the GUI screen (if connected) is in read-only mode, all buttons are disabled except the "Set / Run" key on the front panel and the "Enable" button on the back of the controller. The controller can be switched from the "Idle" state to the "Off", "Enable" and "Set" states.

[0092] 5. The "Set" state is entered from the "Idle" state by turning the "Set / Run" key to the "Set" position. If the key is in the "Set" position when power is applied, the controller must remain permanently in the "Idle" state until the "Set / Run" key is turned to the "Run" position. If the "Set / Run" key is in the "Set" position when the "Idle" state is entered, the key must be turned to "Run" and back to "Set" to enter the "Set" state. In the "Set" state, the GUI functions are available in read / write mode and setting parameters can be changed. All changes are saved to the controller's non-volatile memory (flash, EPROM, etc.) and to the text / config file on the GUI PC. All front panel buttons (except the "Set / Run" key), valves, heater, Peltier and insertion functions remain disabled. The controller can be switched from the "Set" state to the "Off", "Idle" and "Service" states.

[0093] 6. The "Idle" state is entered from the "Set" state if the "Set / Run" key is turned to the "Run" position.

[0094] 7. Enter "Service" state from "Settings" by pressing the "Enable" button on the rear panel of the controller. If the "Enable" button is pressed while entering the "Service" state, it must be released and pressed again to enter the "Service" state from the "Settings" state. Upon entering the "Service" state, the controller must read all current settings information stored in the non-volatile memory (flash, EPROM, etc.) of the controller. In the "Service" state, the insert function is enabled to power the heater and Peltier and temperature feedback control is enabled. All GUI and front panel control buttons are active in the "Service" state. The controller can enter the "Shutdown" and "Idle" states from the "Service" state.

[0095] 8. In the "Service" state, interlock and limit conditions are monitored and if the operation violates a safety condition, (a) a GUI pop-up message should display: "Operation violates at least one safety limit and can be dangerous. Press "OK" to continue operation in the "Service" state or press "Cancel" to return, and (b) the corresponding button on the controller should start flashing at a 2 Hz frequency. Pressing "OK" in the "Service" state should return the controller to the "Idle" state. Pressing "Cancel" in the "Service" state should return the controller to the "Settings" state.

[0096] 9. Enter "Idle" state from "Service" state by turning the "Settings / Run" key to the "Run" position.

[0097] 10. Enter "Enabled" state from "Idle" state by pressing the "Enable" button on the rear panel of the controller. If the "Enable" button on the rear panel is pressed during power-up, it must be released and pressed again to enter the "Enabled" state from the "Idle" state. Upon entering the "Enabled" state, the controller must read all current settings information stored in the non-volatile memory (flash, EPROM, etc.) of the controller.

[0098] 11. In the "Enabled" state, the heater / Peltier is powered, temperature and pressure readbacks are monitored, and interlock conditions are checked. The controller should remain in the "Enabled" state as long as any enabled readback is outside of tolerance or any enabled interlock condition is not met. In the "Enabled" state, the inject button on the GUI and the inject button on the front panel of the controller are disabled. In the "Enabled" state, only retract operation of the GIS is allowed. If the GIS is extended when the controller enters the "Enabled" state, it should remain in the extended position. The GIS can be retracted by pressing the corresponding button on the GUI or on the front panel of the controller, but extension is disabled. The controller can enter the "Shutdown", "Service", "Idle", and "Ready" states from the "Enabled" state.

[0099] 12. Enter "armed" state from "ready" or "run" state when at least one enabled readback is out of tolerance or at least one enabled interlock becomes active. If the controller enters "armed" state from "run" or "ready" state, the GIS position does not change. If the controller enters "armed" state from "ready" or "run" state, all injection valves should be closed and an error message corresponding to the reason for entering "armed" state must be displayed.

[0100] 13. Enter "service" state from "armed" state by turning the "set / run" key to the "set" position.

[0101] 14. Enter "ready" state from "armed" state when all readbacks are within tolerance and interlocks are inactive for at least 10 seconds.

[0102] 15. Enter "service" state from "ready" state by turning the "set / run" key to the "set" position.

[0103] 16. Enter "run" state from "ready" state by pressing one or more "inject / off" buttons on the GUI or front panel of the controller and opening the corresponding injection valves. The controller can enter "off, "service," "ready," and "armed" states from "run" state.

[0104] 17. Enter "service" state from "run" state by turning the "set / run" key to the "set" position. If any injection valve is open when entering "service" state from "run" state, such valve should remain open. If the GIS is extended when entering "service" state from "run" state, the GIS should remain extended.

[0105] 18. Enter "ready" state from "run" state by pressing the inject button on the GUI or front panel of the controller and closing all injection valves.

[0106] 19. Enter "idle" state from "armed," "ready," or "run" state when one of the hardware limits of the temperature or pressure readbacks is exceeded or an abnormal hardware condition is detected.

[0107] Controller and GUI behavior in "idle" and "armed" states

[0108] The following are various examples of state changes related to "idle" and "armed" states.

[0109] 1. Controller enters "idle" state upon power-up: Controller is powered on, all injection valves are closed, the GIS is retracted, the heaters / Peltiers are disabled, and the readback and interlock indicators are "armed."

[0110] 2. When the controller is in "Idle" state and the Set / Run key is in "Run" position and the GUI application is started and connected, the GUI screen is read-only: temperature, pressure and status are read back, but the control buttons of the GUI are disabled. The "Settings" function of the GUI is read-only: parameters can be read, but cannot be modified or uploaded to the controller.

[0111] 3. When the controller is in "Idle" state and the "Set / Run" key is in "Run" position, all buttons on the controller are disabled.

[0112] 4. When the controller is in "Idle" state, turning the "Set / Run" key to "Settings" position, the controller enters "Settings" state. After connecting with the GUI application, the "Settings" function of the GUI is available for read / write: parameters can be changed and uploaded to the controller. In "Settings" state, the injection valve buttons and the GIS insertion button on the GUI are disabled. Turning the Set / Run key to "Run" in "Settings" state should close all valves, retract the GIS and return the controller to "Idle" state.

[0113] 5. When the controller is in "Idle" state and the "Set / Run" key is in "Settings" position, the physical buttons on the front panel of the controller are enabled in "Service" state. Pressing and holding a physical button for 3 seconds or more will make the button flash when the button is released, and if the GUI is connected, a confirmation dialog will pop up on the GUI. Pressing and holding the same button repeatedly for 3 seconds or more will open the corresponding valve and change the button indication on the GUI to "Open", regardless of the interlock and read-back status. The insertion of the GIS is similarly a 3-second press-and-hold operation. When a valve is opened or a GIS is inserted, pressing the same button repeatedly for any time should close the valve or retract the GIS. Turning the Set / Run key to "Run" position when the controller is in "Idle" state should close all valves, retract the GIS and return the controller to "Idle" state.

[0114] 6. When the controller is in "Idle" state and the Set / Run key is in "Settings" position, the "Reset" button on the back of the controller is enabled. If the "Reset" button is pressed and held for 3 seconds or more, the controller can be switched to "Service" state when the button is released.

[0115] 7. Turning the "Set / Run" key from "Service" state to "Run" position can switch the controller to "Enabled" state or "Ready" state.

[0116] 8. When the controller is in "Service" state, the GUI buttons and the front panel controller buttons are operable in "Service" state.

[0117] 9. When the controller is in the "armed" state, if the temperature and / or pressure readbacks are outside the tolerance for any particular tank, the LED on the corresponding button on the controller should flash, the "temperature" and "pressure" indicators next to the virtual button on the GUI should change to red, and the "ready" LED on the front panel of the controller should flash. Once the temperature / pressure readback values are within the tolerance, the LED in the corresponding button on the front panel should extinguish, the "temperature" and "pressure" indicators next to the corresponding on / off button on the GUI should change to green. If any other interlocks are armed, the "ready" LED on the front panel of the controller should continue to flash. If all readbacks are within the tolerance and no interlocks are armed, the "ready" LED changes to "lit" and the controller switches to the "ready" state.

[0118] 10. If the controller is powered on and not connected to the GUI, the controller should operate normally in the "run" or "set" state using the set information stored in the controller based on the "set / run" key position and front panel button controls. Normal operation of the controller should be initiated by turning the "set / run" key to the "set" position, pressing the "reset" button for 3 seconds or more, waiting for the tank temperature and pressure readbacks of the heating / cooling / Peltier controls to be within the tolerance, and once all armed interlocks are in the "armed" state, they can be operated normally using the front panel buttons.

[0119] 11. If the controller loses connection to the GUI while operating in the "run" state, it should continue to operate normally through the front panel button controls.

[0120] 12. If the controller loses connection to the GUI while operating in the "set" state, it should close the injection valve and switch to the "idle" state. Returning from the "idle" state to the "armed" state is done by manually turning the run / set key to the "set" position and pressing the "reset" button for 3 seconds or more. After checking that all temperature and pressure readbacks are within the tolerance and no interlocks are armed, return to the "ready" state.

[0121] 13. If the GUI loses connection to the controller, it should: (a) change the connection status message to "lost", (b) stop drawing the graphs, (c) remain operational in the view only mode, and (d) keep checking the connection to the controller every few seconds.

[0122] 14. When the GUI software starts, it should display the connection status "establishing" and check the connection to the controller. If there is no connection, it should display the connection status message "lost" and remain operational in the view only mode while checking the connection to the controller every few seconds.

[0123] 15. When the GUI software first connects to the controller after the software is started, it should display the connection status "Validating", read the GIS type and set values from the controller, and compare them to the values stored on the computer. If the GIS type and set values are the same, the GUI should display the connection status "Connected" and operate normally. If the GIS type and set values in the controller do not match the information stored in the PC GUI software, a message "GUI / controller mismatch" should be displayed and three options given: (a) upload the configuration from the controller to the GUI; (b) download the configuration from the GUI to the controller; (c) compare the controller and GUI configurations. Options (a) and (b) should save the controller and GUI configurations as text files for future reference and continue, while (c) should open both files in Notepad++ and start the "Compare" plugin.

[0124] Controller and GUI behavior in "Ready" and "Run" states.

[0125] Below are various examples of state changes related to the "Ready" and "Run" states.

[0126] 1. In the "Ready" state, left-clicking the GUI jet button or pressing the physical button on the controller front panel should open the corresponding valve if (a) the GIS is extended, (b) the valve is closed, and (c) no other incompatible valves are open. Opening the valve should (a) toggle the LED in the physical button on the controller front panel to "on", (b) change the color of the GUI button from "dark" to "bright", and (c) change the word on the GUI from "off" to "jet".

[0127] 2. In the "Ready" state, when the jet valve is closed and the GIS is retracted, left-clicking the GUI jet button or pressing the physical jet button on the controller front panel should (a) pop up a dialog box with options (a) open the jet valve without extending the GIS, (b) extend the GIS and open the jet valve after extension, and (c) cancel the operation; (b) make the LED on the controller's jet button and the LED on the extend button flash at a 2 Hz frequency. Pressing the physical jet button on the controller front panel in this state should open the valve without extending the GIS and the pop-up dialog box should disappear, pressing the "extend" button should extend the GIS and open the jet valve and the pop-up dialog box should disappear, and pressing both buttons should cancel the operation and the pop-up dialog box should disappear.

[0128] 3. In the "Ready" state, opening any jet valve should switch the controller from "Ready" to "Jet" state.

[0129] 4. In the "Jet" state, closing all jet valves should switch the controller from "Jet" to "Ready" state.

[0130] 5. In the "Jetting" state, left-clicking the GUI's Jetting button or pressing the physical button on the controller front panel corresponding to opening a jetting valve should close the valve. Closing the valve should (a) toggle the LED on the physical button on the controller front panel to "off, (b) change the color of the GUI button from "bright" to "dim," and (c) change the word on the GUI button from "Jetting" to "Off."

[0131] 6. In the "Ready" state, left-clicking the GUI's Cold Sweep button should execute a cold sweep cycle. In the "Jetting" state, left-clicking the GUI's Cold Sweep button is ignored.

[0132] 7. In the "Jetting" state, left-clicking the GUI's Hot Sweep button should execute a hot sweep while the valves are closed. If multiple (compatible) jetting valves are opened before or after the Hot Sweep button is pressed, the hot sweep is executed when the last jetting valve is closed, regardless of the order in which the jetting valves were opened. In the "Ready" state, pressing the GUI's Hot Sweep button is ignored.

[0133] 8. In the "Ready" state, left-clicking the GUI's Extend / Retract button or pressing the physical Extend / Retract button on the controller front panel should (a) extend the GIS if it is retracted, causing the LED on the "Extend / Retract" button to flash at a frequency of 0.5 Hz during extension and toggle the LED to "on" when the GIS is extended, and (b) retract the GIS if it is extended, causing the LED on the "Extend / Retract" button to flash at a frequency of 0.5 Hz during retraction and toggle the LED to "off" when the GIS is retracted.

[0134] 9. In the "Jetting" state, if the GIS is extended with at least one jetting valve open, then left-clicking the GUI's Extend / Retract button or pressing the physical Extend / Retract button on the controller front panel should (a) pop up a dialog with the following options: (a) retract the GIS without closing the jetting valves, (b) close the jetting valves first and then retract the GIS, (c) cancel the operation; (b) cause the LEDs on the physical "Jetting / Off" buttons corresponding to the open valves and the "Extend / Retract" button on the controller front panel to flash at a frequency of 2 Hz. If the flashing "Jetting / Off" button is pressed, the jetting valves should close, the GIS should retract, and the pop-up dialog should disappear. If the flashing "Extend / Retract" button is pressed, the GIS should retract without closing the jetting valves, and the pop-up dialog should disappear. If both the flashing "Jetting / Off" button and the flashing "Extend / Retract" button are pressed simultaneously, the operation will be canceled, and the pop-up dialog should disappear.

[0135] 10. In the "JETTED" state of the GIS retracted, pressing the GUI or physical "EXTEND / RETRACT" button should extend the GIS to cause the LED on the "EXTEND / RETRACT" button to flash at a frequency of 0.5 Hz during extension and switch the LED to "ON" when the GIS is extended.

[0136] Controller and GUI behavior in the "SETUP" and "SERVICE" states.

[0137] Below are various examples of state changes related to the "SETUP" and "SERVICE" states.

[0138] 1. When the controller is in the "SETUP" or "SERVICE" state, the front panel buttons operate in "SERVICE" mode: holding a physical button for 3 seconds or more will cause the button to flash on release and, if the GUI is connected, a confirmation dialog will pop up on the GUI. Repeatedly pressing and holding the same button for 3 seconds or more will open the corresponding valve and change the button indication on the GUI to "OPEN", regardless of interlock and readback state. Insertion of the GIS is likewise a two-stage 3-second press-and-hold operation. When the valve is open or the GIS is inserted, repeatedly pressing the same button for any period of time should close the valve or retract the GIS.

[0139] 2. When the controller is in the "SETUP" or "SERVICE" state and the GUI is connected, the "SETUP" function of the GUI application can be used to read / write: parameters can be changed and uploaded to the controller. In the "SETUP" state, the JET and GIS INSERT buttons on the GUI operate in "SERVICE" mode: if the GUI button is pressed for 3 seconds or more, releasing the button opens a pop-up dialog to confirm opening the JET valve or extending the GIS. While the dialog is open, the corresponding button on the controller should start flashing rapidly. When confirmed, the valve should open and / or the GIS should extend, regardless of readback and interlocks; the light on the button should change to "ON". When the valve is open or the GIS is inserted, repeatedly pressing the same button for any period of time should close the valve or retract the GIS; the light should return to the state of its corresponding current state.

[0140] 3. When the controller is in the "SETUP" or "SERVICE" state, left-clicking the "COOLING PURGE" or "HEATING PURGE" buttons on the GUI is performed in the same manner as in the "READY" and "JETTED" states.

[0141] Controller front panel button LEDs and indicators

[0142] Below are various examples of state changes related to changes using the control panel.

[0143] 1. The Run / Service LED on the front panel is "off" in the "Idle" state, flashes at 0.5 Hz in the "Set" and "Service" states, flashes at 1 Hz in the "Enable" state, and is "on" in the "Ready" and "Jet" states.

[0144] 2. The Ready LED on the front panel flashes at 0.5 Hz in the "Idle" and "Set" states, flashes at 1 Hz in the "Service" and "Enable" states if one of the enabled back reads is out of tolerance or one of the enabled interlocks is enabled, is "on" in the "Service" state if all enabled back reads are within tolerance and no enabled interlocks are enabled, and is "on" in the "Ready" and "Jet" states.

[0145] 3. The LED in the GIS Extend / Retract button is "off" when the GIS is retracted, "on" if the GIS is inserted, flashes at 0.5 Hz when the GIS is being inserted or retracted, flashes at 1 Hz if the GIS is in an "error" state (i.e. neither inserted nor retracted or both inserted and retracted for a period of time beyond the insert / retract time), and flashes at 2 Hz if retract is attempted with one or more jet valves open and no acknowledgement is given.

[0146] 4. The LED in the "Jet / Off" button on the controller front panel is "on" when the valve is open, flashes at 0.5 Hz for 3 seconds after being held down in "Service" or "Set" mode, flashes at 1 Hz in "Service" mode or "Enable" mode if the temperature or pressure back read of the enabled corresponding tank is out of tolerance, flashes at 2 Hz if the valve is attempted to be opened in the "Ready" or "Jet" state with the GIS retracted and no acknowledgement is given, and is "off" at all other times.

[0147] Software Safety Features

[0148] The following are various examples of state changes related to safety features.

[0149] 1. All buttons are connected through a 100 mSec "debouncer" that will ignore button state changes shorter than 100 mSec;

[0150] 2. All interlocks are connected through a 100 mSec "debouncer" that will ignore button state changes shorter than 100 mSec;

[0151] 3. The temperature and pressure readings of the GUI graphics are "real-time" as per the controller's sampling rate, but tolerance compliance or non-compliance is "filtered" over 2 seconds.

[0152] 4. The "Enable" button must be "released" and converted to "active" state to switch the controller from "Idle" to "Enable" state or from "Setup" to "Service" state.

[0153] 5. The "Setup" key must be in "Run" position and converted to "Setup" state to switch the controller from "Idle" to "Setup" state and from "Enable" or "Run" to "Service" state.

[0154] 6. All setup parameters are stored in the controller. Actual parameters are read from the controller to be displayed on the GUI.

[0155] 7. All calculations and decisions are made within the controller; the GUI is only used as an indicator / monitor. All states and graphs are read from the controller to be displayed on the GUI.

[0156] 8. The internal operation of the controller is in temperature and / or pressure A / D bits, which allow a range of 0 to 1023. Conversion from bits to temperature and / or pressure units is done in the GUI software on the PC only to facilitate manual reading.

[0157] 9. The internal operation of the temperature control is in D / A bits, which allow a range of 0 to 255.

[0158] Setup function

[0159] The following describes when the controller is in "Idle", "Enable", "Ready" and "Fire" states, or if the GUI is disconnected from the controller, right-click on the corresponding GUI element to open the following configuration popup in read-only mode. When the controller is in "Setup" or "Service" state and the GUI is connected to the controller, right-click on the corresponding GUI element to open the following configuration popup in read / write mode, any changes are stored in the configuration file and uploaded to the controller.

[0160] 1. Temperature units: K, C, F - for all temperature settings and readbacks; unit change should convert all settings and readback values.

[0161] 2. Pressure units: Mbar, Torr, Pa - for all pressure settings and readbacks; unit change should convert all settings and readback values.

[0162] 3. Chamber vacuum HW interlock: E - enabled; D - disabled;

[0163] 4. Tank vacuum HW interlock: E - enabled; D - disabled;

[0164] 5. Insert HW interlock: E - enabled; D - disabled;

[0165] 6. Chamber vacuum readback: A - enabled; D - disabled; default is "D" (not used now)

[0166] a. Voltage - pressure table should be stored; chart colors should be selectable

[0167] 7. Chamber vacuum minimum: lowest chamber vacuum for operation (only when readback is A)

[0168] 8. Chamber vacuum maximum: highest chamber vacuum for operation (only when readback is A)

[0169] 9. Nozzle pressure readback: A - enabled; D - disabled; default is "D" (not used now)

[0170] a. Voltage - pressure table should be stored; chart colors should be selectable 10. Nozzle pressure minimum: lowest nozzle pressure for operation (only when readback is A) 11. Nozzle pressure maximum: highest nozzle pressure for operation (only when readback is A) 12. Reservoir settings for three reservoirs (H - heated, C - cooled, P - Peltier)

[0171] a. Minimum readback temperature; this is the thermistor range definition

[0172] b. Maximum readback temperature; this is the thermistor range definition

[0173] c. Voltage - temperature (thermistor readback) table

[0174] d. Overheat limit: maximum temperature for operation; this limit puts the controller into idle state, error message

[0175] e. Undercool limit: minimum temperature for operation; this limit puts the controller into idle state, error message

[0176] 13. Gas settings for four precursor reservoirs:

[0177] a. Reservoir ID - read-only field

[0178] b. Gas: precursor name or chemical formula "0" disabled

[0179] c. Color: defines color of on / off button on GUI and color of temperature graph

[0180] d. Reservoir type: H (heated), C (cooled), P (Peltier), A (ambient)

[0181] e. Temperature setpoint: operating temperature

[0182] f. Temperature tolerance: operating temperature range; default + / - 1 C

[0183] g. Precursor pressure readback: A - enabled; D - disabled; default is "D" (not used now)

[0184] i. A voltage-pressure table should be stored, the chart color should be selectable

[0185] h. Precursor pressure minimum: lowest nozzle pressure for operation (only when readback is A)

[0186] i. Precursor pressure maximum: highest nozzle pressure for operation (only when readback is A)

[0187] j. Compatibility: ID of the tank that can be opened simultaneously with the current tank

[0188] Open delay: minimum time after closing the jet valve on another tank before the current tank can be opened; 0 seconds to 1000 seconds

[0189] l. Open purge skip delay: minimum time after closing the jet valve on another tank to skip the open purge; 0 seconds to 1000 seconds

[0190] m. Open purge: yes / no; if "yes", a cold purge cycle is performed before opening the jet valve on the tank; if "no" no purge cycle

[0191] n. Open purge duration: 10 seconds to 1000 seconds. This setting overrides the duration in the cold purge cycle settings

[0192] o. Close purge: hot / cold / no; if "hot" or "cold", a corresponding purge cycle is performed after closing the tank, if "no" no purge cycle is performed

[0193] p. Close purge duration: 10 seconds to 1000 seconds. This setting overrides the duration in the hot purge cycle settings

[0194] q. Charge: mass of the precursor charge, grams

[0195] r. Consumption rate: grams / second

[0196] s. "Reset" button for the "open time" and "consumption" counters

[0197] 14. Extension / retraction settings:

[0198] a. Extension readback: 1 - enabled high; 0 - enabled low; D - disabled

[0199] b. Retraction readback: 1 - enabled high; 0 - enabled low; D - disabled

[0200] c. Extension / retraction action timer, range 1 second - 30 seconds, default value 5 seconds

[0201] d. Extend purge duration (in seconds, "0" to disable); time period to perform a cold purge cycle during GIS insertion. If both tank open and extend purge are specified, extend purge is performed first, then tank open purge

[0202] e. Retract purge duration (in seconds, "0" to disable); time period to perform a cold purge cycle during GIS retraction. If both tank close purge and retract purge are specified, tank purge is performed first, then retract purge

[0203] 15. Nozzle settings:

[0204] a. Temperature color: Define color of nozzle temperature graph

[0205] b. Temperature setpoint: Nozzle operating temperature

[0206] c. Temperature tolerance: Operating temperature range; default + / - 1C. If nozzle temperature is outside tolerance, tank valve does not open and "ready" indicator on controller blinks

[0207] d. Minimum readback temperature; this is the thermistor range definition

[0208] e. Maximum readback temperature; this is the thermistor range definition

[0209] f. Voltage-temperature (thermistor readback) table

[0210] g. Overheat limit: Maximum temperature of operation; this limit puts controller into idle state, error message

[0211] h. Undercool limit: Minimum temperature of operation; this limit puts controller into idle state, error message

[0212] i. Nozzle pressure readback: A - enabled; D - disabled; default value is "D" (not used now)

[0213] i. A voltage-pressure table should be stored, chart color should be selectable

[0214] j. Nozzle pressure minimum: Lowest nozzle pressure of operation (only when readback is A)

[0215] k. Nozzle pressure maximum: Highest nozzle pressure of operation (only when readback is A) 16. Cold purge cycle settings:

[0216] a. Purge tank ID and type; default values are 4 and ambient

[0217] b. Delay: Time to delay opening purge tank valve after closing jet valve; 0 milliseconds to 10,000 milliseconds

[0218] c. burst: time to open purge tank jet during burst, 1 to 10,000 milliseconds

[0219] d. cycle: time of cycle, 1 to 10,000 milliseconds. Jet is closed after burst until end of cycle. If burst >= cycle, jet remains open during cycle.

[0220] e. duration: duration of cold purge cycle after GUI button is pressed, 10 to 1200 seconds

[0221] 17. Hot purge cycle settings:

[0222] a. purge tank ID and type; default values are 4 and ambient

[0223] b. lead: time to delay closing precursor jet before first opening purge tank jet, 1000 milliseconds to 0 milliseconds

[0224] c. burst: time to open purge tank valve during cycle, 1 to 10,000 milliseconds

[0225] d. cycle: time of cycle, 1 to 10,000 milliseconds. Valve is closed after burst until end of cycle. If burst >= cycle, valve remains open during cycle

[0226] e. duration: duration of hot purge cycle after GUI button is pressed, 10 to 1200 seconds

[0227] 18. Graph and log settings:

[0228] a. time interval to record when one or more tank valves are open. In this case all enabled readbacks and status are recorded. 0.1 seconds, 1 second, 10 seconds.

[0229] b. time interval to monitor for state changes of predefined parameters to record if all tank valves are closed. 1 second, 10 seconds, 30 seconds

[0230] c. readback parameter to check when all tank valves are closed. Radio button selection

[0231] d. number of log files to keep or duration

[0232] 19. Temperature PID settings (for nozzle and each tank):

[0233] a. CV Est — voltage estimation constant

[0234] b. PID control window (0.1....5) x tolerance

[0235] c. PID update rate (msec)

[0236] d. Smoothing constant (0 - no smoothing, 1 - ignore sensor)

[0237] e. I Lim — Integral limit

[0238] f. P - Proportional gain

[0239] g. I - Integral gain

[0240] h. D - Derivative gain;

[0241] Many modifications and alterations will occur to others upon reading and understanding the preceding description. It is intended that the application be constructed: as including all such modifications and alterations insofar as they come within the scope of the appended claims and / or the following claims. In the description herein, numerous specific details are set forth in order to provide a thorough understanding of the embodiments. However, various embodiments can be practiced without the specific details. In other instances, well-known methods, procedures, components, and circuits have not been described in detail so as not to obscure aspects of the embodiments. The foregoing description is not intended to be exhaustive or to limit embodiments of the present application to the precise forms disclosed. While specific embodiments of, and examples for, the application are described herein for illustrative purposes only, various equivalent alterations and modifications will be apparent to others skilled in the relevant arts in view of this description. Accordingly, the various embodiments disclosed herein are by way of example only and are not intended to limit the scope of the application according to the patent statutes, unless such limitations are expressly adapted by the following claims and / or appropriate legal equivalents.

Claims

1. A gas injection system, comprising: a housing configured to house a plurality of precursor reservoirs, the precursor reservoirs comprising one or more precursor materials; a nozzle extending from the housing, the nozzle having a tip configured for insertion into a sample chamber of a material processing apparatus; the precursor reservoirs being fluidly connected to the nozzle to selectively deliver one or more precursor gases into the sample chamber.

2. The gas injection system of claim 1, wherein the housing comprises a plurality of reservoir housings configured to receive the precursor reservoirs.

3. The gas injection system of claim 1, wherein the housing forms a vacuum envelope around the plurality of precursor reservoirs.

4. The gas injection system of claim 2, wherein each reservoir housing comprises an integrated valve to fluidly connect the precursor reservoir disposed in the reservoir housing to the nozzle.

5. The gas injection system of claim 1, wherein the plurality of precursor reservoirs are fluidly connected in series to one or more delivery lines in fluid communication with the nozzle and the sample chamber.

6. The gas injection system of claim 5, further comprising a plurality of three-way valves to sequentially fluidly connect the plurality of precursor reservoirs to the one or more delivery lines.

7. The gas injection system of claim 5, wherein the one or more delivery lines are thermally controlled to prevent condensation of the precursor gases in the one or more delivery lines.

8. The gas injection system of claim 5, wherein the one or more delivery lines are fluidly connected to one or more injection capillaries disposed in the nozzle for delivering the precursor gases into the sample chamber.

9. The gas injection system of claim 8, wherein the nozzle comprises a plurality of injection capillaries for simultaneous injection of a plurality of precursors into the sample chamber.

10. The gas injection system of claim 3, wherein each of the plurality of reservoir housings comprises one or more temperature control elements configured to operate independently of one or more heating elements associated with other reservoir housings to maintain each of the plurality of precursor reservoirs at a temperature selected to sublimate a precursor gas in that precursor reservoir.

11. The gas injection system of claim 1, wherein the nozzle is configured to be maintained under a thermal gradient along a length of the nozzle.

12. The gas injection system of claim 11, wherein the temperature increases toward the tip of the nozzle.

13. The gas injection system of claim 5, wherein the nozzle and the housing are configured to form a vacuum envelope around the precursor reservoirs and the one or more delivery lines.

14. A method for delivering a plurality of precursor gases into a sample chamber of a material processing apparatus, the method comprising: inserting a gas injection system into the material processing apparatus, wherein the gas injection system comprises: a housing configured to house a plurality of precursor reservoirs, the precursor reservoirs comprising one or more precursor materials; a nozzle extending from the housing, the nozzle having a tip configured for insertion into a sample chamber of a material processing apparatus; a nozzle extending from the housing, the nozzle having a tip configured to be inserted into a sample chamber, the precursor reservoirs being fluidly connected to the nozzle; forming a vacuum in the housing around the plurality of precursor reservoirs; individually heating the plurality of gas precursor reservoirs to a temperature sufficient to generate one or more precursor gases from the one or more precursor materials; and selectively delivering one or more precursor gases from the plurality of gas precursor reservoirs into the sample chamber.

15. The method of claim 14, further comprising heating the gas injection system to a temperature sufficient to prevent condensation of the one or more precursor gases and maintaining the temperature.

16. The method of claim 14, wherein the housing comprises a plurality of reservoir housings configured to receive the precursor reservoirs.

17. The method of claim 16, wherein each reservoir housing comprises an integrated valve to fluidly connect a precursor reservoir disposed in the reservoir housing to the nozzle.

18. The method of claim 14, wherein the plurality of precursor reservoirs are fluidly connected in series to one or more delivery lines in fluid communication with the nozzle and the sample chamber.

19. The method of claim 18, wherein the system further comprises a plurality of three-way valves to sequentially fluidly connect the plurality of precursor reservoirs to the one or more delivery lines.

20. The method of claim 19, wherein the one or more delivery lines are thermally maintained to prevent condensation of the precursor gases in the one or more delivery lines.

21. The method of claim 19, wherein the one or more delivery lines are fluidly connected to one or more injection capillaries disposed in the nozzle for delivering the precursor gases into the sample chamber.

22. The method of claim 14, wherein the nozzle is configured to be maintained under a thermal gradient along a length of the nozzle.

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